Continuous process for the distillation and rectification of alcoholic liquids.



V. SLAVICEK.

CONTINUOUS PROCESS FOR THE DISTILLATION AND RECTIFICATION 0F ALCOHOLICLIQUIDS.

APPLICATION FILED OCT. 29,1908.

1,136,559, Patented Apr.20, 1915.

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CONTINUOUS PROCESS FOR THE DISTILLATION AND RECTIFICATION OF ALCOHOLICLIQUIDS.

Specification of Letters Patent.

Patented Apr. 20, 1915.

Application filed October 29, 1908. Serial No. 460,107.

To all whom it may concern Be it known that I, VICTOR SLAViEK, a subjectof the Austro-Hungarian Emperor, and resident of Strozzigasse, VIII,Vienna, Austria-Hungary, have invented certain new and usefulImprovements in Continuous Processes for the Distillation andRectification of Alcoholic Liquids, of which the following is aspecification.

The present invention relates to a process for the continuousdistillation and rectification of spirits obtained by the usual process.The spirits, produced either direct from the mash or from raw spirits orwine, possess always a very unpleasant ordor even if chemical impuritiescannot be traced and the greatest care in the production has prevailed.This odor is created first .by the vapors to be purified passing theconcentrated last-runnings covering the partitions of the rectifyingcolumn and according to the strength of the degree of concentration willbe more or less noticeable. Secondly they are caused by the fact thatthe crude vapors or phlegms, that is all liquids, which remainunvaporized in any part of the apparatus, even if they are freed fromthe fore-runnin gs before entering the rectifying column will becomeimpure during the long purifying process by oxidation through theintaking of air during the irregular working of the apparatus or forinstance the irregular taking in of mash or steam, or bythe irregularcooling ofi", etc. r

The object of this invention is a continuous process for distilling andrectifying alcoholic liquids which obviates the aforesaid defects andassures a complete purificationand the removal of all unpleasant odors.i

The improved process consists mainly in the followingz'lllrst individing the crude vapors. One part of the same is passed through apreliminary purifier from which the boiling-hot phlegms of this part,purified from the fore-runnings are introduced in a fine spray and inone direction into the second part of the crude vapors which is freefrom forerunnings but contains last runnings the alcohol only in vaporform and also absorbs the last-runnings of the crude vapors so thatwithout extra cooling or re-vaporization pure vapors are obtained whilein the rectifying column occurs a reduced con- The second part yieldscentration and a lower level. of the last-runnings. The reactions whichare obtained through this process may be noted from the examples asshown farther on. Second all non-condensed impurities generated orcarried into the rectifying column are returned as vapor to the firstpurifier for heating purposes. Third an exact equalizing and automaticregulating of the pressure in the various parts of the apparatus isobtained by means of a particular circulation.

The accompanying drawing showsin section in a diagrammatic form adistilling and rectifying apparatus for carrying out the above describedprocess.

Material entering through the inlet 1 into the upper part of thedistillation column or still B is practically purified from theforerunnings in B, and leaves at the lower end of the column A through apipe 2. The stream of water vapor flowing into the mash is introducedthrough the pipe 3 at the lower part of the column A and in penetratingthe mash becomes saturated with crude-vapors extracted from the same. Asolid partition 30 closes for the rising steam the direct communicationbetween A and B,whereas the liquid can flow downward through the pipe28. In the upper part of the column A, a part of the crude-vapors insuitable quantity is carried by the pipe connection 4' into the columnBand thence through a similar pipe 5 into the purifier C, D. The directconnection between B and C is closed for the steam as Well as for theliquid by the partition 29, whereas C and D communicate. From the upperpart of the column C, D the volatile fore-runnings escape through the pie 19, whereas the hot alcoholic phlegms, wliich are free fromfore-runnlngs, collect above the partition 29. From here the latter bymeans of the pipe 6 and the sprinkler 6 are brought into the pipe 7 inform of a fine spray in close intermingling with the second unpurifiedpart of the crude-vapors which are free from fore-runnings coming fromthe distillation column A. From pipe 7 the vapors pass to the rectifylngcolumn F which is mounted on the column E provided at the lower partwith a steam inlet 8 and a water, outlet 9. The crude-vapors arerelieved of a great amount of last-runnings adhering thereto in finedrops by introducing the phlegms into pipe 7 in a fine spray and in onedlrection whereby one part of the ill smelling end-products is absorbed,like dust in the air by rain, from the finely sprinkled, downwarddropping hot phlegms and is abstracted with the same in a known way. Thepurification occurs in this manner that the phlegms from the column C ina boiling hot state, inineeting the crude-vapors discharge fromthemselves the alcohol as vapor and absorb, while drizzling downward,from the crude-vapors the last-runnings and become saturated therewith.This mode of purifying the vapors by the hotphlegms is much moreeffective than the purification-by condensation, also from an economicalstand point the saving in cooling, heating and working has to be takeninto consideration. Furthermore, in purifying the crude-vapors byequally strong phlegms a carrying along of the last-runnings, whichusually takes place when boiling alcoholic liquors, is entirely avoided.To prevent the entrance of mash or foam from the distilling column Ainto the pipe 7, or its being carried along by the vapors, a receptacle7 a is provided between the pipe 7 and the column A. By the describedworking manner much purer crude-vapors enter the rectification columnwhich have already lost most of the ill smelling last-runnings whereby avery much lower concentration of the last-runnings and a lower form ofcolumn is required, or in other words it extends over a smaller numberof partition or bottom plates facilitating thereby the rectificationconsiderably. From the column F the already very pure vapors reachthrough the pipe 10 the dephlegmator H and are-here dephlegmated underthe highest possible temperature. The phlegms are returned through pipe16 to the column F and the rest of the vapors reach through pipe 11 thecondenser J where again condensation takes place at the highestvpossible temperature. The higher the temperature of the dephlegmationand the condensation are, the purer and more odorless the fine-productobtained will be. The-alcoholic phlegms are conducted througlrthe pipe12 'into the column K and are here once more rectified by steam, let inthrough the pipe 13. The fine-product or spirits is drawn off from thecolumn K v by the pipe 15, Whereas the discharged volatile productscommingle with the non-condensed parts coming from the condenser I andare conducted back in vapor form, containing all their heat, through thepipe '14 into the head-product purifier O, D on a place of less counterpressure, where they act as heating means and are subjected to a commontreatment with the first part of the crude-vapors. In this manner allprimeproducts or fore-runnings and the volatile products generated bythe process are conducted circulating in vapor form to the universalpurifier D. The noncondensed parts escaping therefrom through the pipe19, are again dephlegmated in Grand are taken off finally through pipe21. The phlegms of G are continuously returned partly through the pip'e17-to the head-product purifier D I not, even if the handling of theapparatus should become irregular from one source or the other.

To prevent impure vapors penetrating through the pipe 14; into the finalpurifier column K, a back-pressure valve is provided in this pipeconnection. I

An increase of pressure in column A, B is followed by a respectiveacceleration of the processes in column E, F and by a nonsuflicientaction of the apparatus H, I and K which action on account of theconnection through pipe 14: is also transmitted to the head-productpurifier C, D. In the same manner an undesirable change of the pressurein any one part of the apparatus acts disturbingly on all the otherparts. It is therefore of great importance to regulate the vaporizationin column A according to the pressure in columns E and Fand condenser Iand dephlegmator H in such a manner that occurring pressure variationsare automatically regulated. According to the present invention this iseffected in an extraordinarily eflicient way by the steam regulator L ofordinary construction, which regulates the steam inflow in the pipe 3according to the steam pressure in pipe 7. In the drawing this regulatoris shown as a diaphragm regulator consisting of a lower condensingreceptacle 9 which is connected by the pipe-7c to the pipe 7 and bymeans of the nozzle 8 with the diaphragm compartment (1 and thediaphragm m. The raising or lowering'of the diaphragm m according to theincrease or decrease of steam pressure in the pipe 7 respectively in thecolumns A and E, F or in the column C, D is transmitted by means of therod 1? and the double-arm lever 0 to the rod u manipulating the valve'1), whereby the steam inlet through the pipe 3 to A is regulatedaccording to the prevailing pressure in the interior of the columns. Bythe peculiar locatior of the steam inlet and thereby the pressure in thecolumn A is regulated from a spot, the pressure of which is equallygoverned from all parts of the apparatus in such a manner, that if thereoccurred on any one point an the regulator L unfavorable change ofpressure, it Will change the pressure in the column A so that theequilibrium in the circulation is restored. From the same regulator thesteam inlet into any other part can be regulated in a like effectivemanner; at any disturbance of the pressure through the action of theregulator an automatic restoring of the pressure in the circulationtakes always place.

For a regular working of the entire apparatus it is finally imperativeto regulate the quantities of the unclean or partly cleaned liquorsintroduced into the parts according to the quantity of alcohol leavingthe column at the same time. Then, should, during a longer period morefine-spirits have been let off through the pipe 15 than for example theamount of phlegms flowing in through the pipe 6, the end-runnings willshow themselves in the rectifying column in too high a column or viceversa. Hereby the purity of the product becomes subjected to greatvariations. It has now been determined that the temperature in thecolumn E, F is a good rule for measuring the right proportions betweenthe quantities of fine spirits taken off at 15, and the new quantity ofliquor conducted at the same time into the various parts of theapparatus, and which can be used for an exact reciprocal regulation ofthe same.

In the drawing, in a constructional form, is shown the device forregulating the quantity of the phlegms passing through the pipe 6, whicharrangement is very effective as thereby indirectly, at the same time,the quantities of the end-products of the head or fore-runnings carriedinto the column E, F, which fore-runnings flow off through the pipe 8,as well as the pressure in the columns A, C, B, D, is accordinglyregulated.

On that part of the rectifying column which is subjected to the greatestvariations in temperature, a closed, fiat expansion case or capsule 22is provided. The case 22 is filled with a suitable liquor, bears on oneside on the wall 26 and is connected to a rod 23 which actuates thetwo-arm lever 24. The latter, by means of the arm 24', actuates the cock25 interposed in the pipe connection 6. At rising temperature thecapsule 22 expands. presses the rod 23 outward and opens thereby, bymeans of the levers 24, 24 and the cock 25 the pipe connection 6 moreand more. This causes more phlegm to run over to E, the temperaturefalls, the capsule 22 contracts and closes the pipe connectiongradually. The sliding back of the rod 23 is accelerated by a spring 27.In the same manner the inflow of the mash into column A and the outflowof the water, etc., of the forerunnings can be regulated.

Through the conduit there will be introduced into the distilling columnA B every hour about 500 liters of a molasses mash of about 12" Baum andof the following composition ethyl alcohol 8%, fore-runnings 0.25% (ofaldehyde 0.15%, other volatile products 0.1%), water 80%, last-runnings,products 0.25%, of which 0.2% is amyl alcohol, 11.5% organic andinorganic salts. To the mash flowing down over the bottom of the columnA B there will be conducted through pipe 3 steam at 5 atmospheres,corresponding to 154 C. in a counterflow, which steam drives out thealcohol, the fore-runnings and a part of the last-runnings. At the pipe2 there pass out each hour about 4200 liters of slop, containing onlyabout 6% of organic substance (salt). The mean temperature in column Aamounts to 103 (1., in B 100 C. Of the 400 liters of pure ethyl alcoholintroduced through inlet 1, there pass over through 5rabout 300 litersin the form of vapor and laden with preliminary products to C, D, wherethere prevails a mean temperature of 841 C. and a pressure of about 1600mm. On the other hand through 7 a and 7 there pass over every hour about100 liters in the form of vapor, which contain no fore-runnings but docontain the last-runnings in the form of finely divided droplets. Tothese vapors there will be conducted through 6 the phlegms or crudevapors free from fore-runnings coming from C, D and having a temperatureof 82 C. and a content of 50% of ethyl alcohol through the spray 6, andbetween these there takes place the change described above. Thepreferred temperature at the place where the conduit goes out from thepipe 7 is 8 1 C. From 7 there passes a very pure vapor with 35% alcoholinto the rectifying column F, while the fore-runnings flowing oil to Econtain nearly all the lastrunnings and about 50% ethyl alcohol. Intothe column E, there is introduced through 9 steam at 5 atmospheres,while at 8 there flow 0H per hour 400 liters of water, containing thewhole of the last-runnings. There prevails a normal temperature of 86C., and this falls on its way to the highest floor of the column Fsuccessively to 81.5 C. The vapors passing out through 10 containalready 96. 1% of ethyl alcohol and are dephlegmated in the dephlegmatorH at 70.5 (7., the vapors leaving H are condensed in J at 77 C. andthese phlegms are again rectified in 12 by steam at 140 C. introduced at13. At 15 there flows oil continually (hourly) a quantity of about 365liters of refined alcohol with a content of 97% ethyl alcohol. Theproducts not condensed in the columns F. H. J and K are carried backthrough 14 at a temperature of 81 (1. into fore-runnings purifier C, D,as heating agent. The volatile products escaping from the purifiercolumn D through 19 areagain dephlegmated at G at 70 C. From the mostvolatile products coming out at 21 there is obtained an hourly quantityof about 32 liters of a condensate, consisting of 3% aldehyde and 93%alcohol, while the remainder is other volatile products speciallyesters. The condensed superfluous fore-runnings products can be let offat 20, while every hour about liters flow back through 17 to D.

At all points of the plant there are placed thermometers and pressuregages so that the temperatures and pressures can easily be observed. Thespecific weights of the distillates are determined by areometers. Onstarting the plant the worl; iscarried on by regulating the steam inletat 3, 9 and 15 and the cook 16, until the conditions of temperature,pres sure and passage are attained. After that the whole plant regulatesitself perfectly by means of the arrangements L and 2,2 in the Waydescribed above.

When the apparatus is once started, one need do nothing further inmanipulating the samef, as the entire process will regulate itsel Thedescribed device for carrying out diss tillation assures the productionof a very pure product at an automatic regulated running of theapparatus at a continuous working.

What I claim as my invention and desire to secure by Letters Patentis 1. The process for the continuous distillation and rectification ofalcoholic liquids,

which consists in dividing the alcoholic raw vapor into two portions,purifyingthe noncooled phlegms of one portion ofthe head products, andintroducing the same immediately at the beginning of the rectificationinto the alcoholic raw vapor of the second portion. i

2. The process forthe continuous distillation and rectification ofalcoholic liquids,

- which consists in dividing the alcoholic raw vapor into two portions,purifying the noncooled phlegms of one portion of the head products, andintroducing the same immediately at the beginning of the rectificationinto the alcoholic raw vapor of the second portion, previously deprivingthe said portion'of the head products but leaving the tail products.

3. The p ocess for the continuous distillation and rectification ofalcoholic liquids, which consists in dividing the alcoholic raw vaporinto two portions, purifying the non cooled phlegms of one portion ofthe head products, and introducing the same immediately at the beginningof the rectification into the alcoholic raw vapor of the second portion,previously depriving the said portion of the head products but leavingthe tail products, and utilizing the mutual contact to vaporize thephlegms.

masses 4:- The process for the continuous distillation and rectificationof alcoholic liquids, which consists in dividing the alcoholic raw vaporinto two portions, purifying the non cooled phlegms of one portion ofthe head products, and introducing the same immediately at the beginningof the rectification into the alcoholic raw vapor of the second portion,previously depriving the said portion of the head products but leavingthe tail products, and utilizing the mutual contact to vaporize thephlegms, and impregnating the same with the tail products.

5. The process for the continuous distillation and rectification ofalcoholic liquids, which consists in dividing the alcoholic raw vaporinto two portions, purifying the noncooled phlegms of one portion of thehead products, and introducing the same immediately at the beginning ofthe rectification which. consists in dividing the alcoholic raw vaporinto two portions, purifying the noncooled phlegms of one portion of thehead products, and introducing the same immediately at the beginning ofthe rectification into the alcoholic raw vapor of the second portion,previously depriving the said portion of the head products but leavingthe tail products, and utilizing the mutual contact to'vaporize thephlegms, and impregnating the same with the tail products, preventingthe same from becoming saturated with alcohol, then passing thealcoholic vapor into a rectifying column.

7. The process for the continuous distilla tion and rectification ofalcoholic liquids, which consistsin'dividing the alcoholic raw vaporinto two portions, purifying the noncooled phlegms of one portion of thehead products, and introducing the same immediately at the beginning ofthe rectification into the alcoholic raw vapor of the second portion,previously depriving the said portion of the head products but leavingthe tail products, and utilizing the mutual contact to vaporize thephlegms, and impregnating the same with the tail products, preventingthe same from becoming saturated With alcohol, then passing thealcoholic vapor into rectifying column, then returning the impurities invapor form to utilize the ,heat thereof.

8. The process for the continuous distillation and rectification ofalcoholic liquids, which consists in dividing the alcoholic raw vaporinto two portions, purifying the noncooled phlegms of one portion or"the head products, and introducing the same immediately at the beginningof the rectification into the alcoholic raw vapor of the second portion,previously depriving the said portion of the head products but leavingthe tail products, and utilizing the mutual contact to vaporize thephlegms, and impregnating the same with the tail products, preventingthe same from becoming saturated with alcohol, then passing thealcoholic vapor into a rectifying column, and preventing the impuritiesfrom entering the rectifying column.

9. A process for the continuous distillation and rectification ofalcoholic liquids wherein the crude alcohol vapors are divided into twoparts, one containing all fore-runnings, one free from fore-runnings,the boiling phlegms of.the first part, purified from the fore-runnings,are led in a fine spray in rain form and in one direction into thesecond part of the crude vapors which is free from fore-runnings, andthat the vapors leaving the mixing compartment are rectified,dephlegmated and condensed.

10. A process for the continuous distillation and rectification ofalcoholic liquids wherein the crude alcohol vapors are divided into twoparts, one containing all fore-runnings, the other free fromforerunnings, the boiling hot phlegms of the first part purified fromthe fore-runnings, are led in a fine spray or rain form and in onedirection into the second part of the crude vapors which is free fromfore-runnings, that the vapors leaving the mixing compartment arerectified and that for the purpose of freeing the same' of all odors andcarried along impurities, the same are at the possible highesttemperature dephlegmated and condensed.

11. A process for the continuous distillation and rectification ofalcoholic liquids wherein the crude alcohol vapors are divided into twoparts, one containing all fore-runnings, the other free fromforerunnings, the boiling hot phlegms of the first part, purified fromthe fore-runnings are led in a fine spray or rain form and in onedirection into the second part of the crude oil vapors which is freefrom forerunnings, that the vapors leaving the mixing compartment arerectified and for the purpose of freein the same of all odors andcarried along lmpurities are at a possible highest temperaturedephlegmated and condensed and that the non-condensed parts in vaporform and containing all their heat are conducted into a zone of thepreliminary purifier, which zone is free fromany injuriouscounter-pressure and are sub ected in circulation under automaticpressure regulation between these parts of the apparatus to acooperative treatment with the first part of the crude vapors.

12. A process for the continuous distillation and rectification ofalcoholic liquids wherein the crude alcohol vapors are divided into twoparts, one containing all fore-runnings, the other free fromforerunnings, the phlegms of the first'part purified from thefore-runnings are led in a fine spray or rain form and in one directioninto the second partof the crude vapors which is free fromfore-runnings, the vapor leaving the mixing compartment are rectifiedand for the purpose of freeing the same of all odor and carried alongimpurities are at a possible highest temperature dephlegmated andcondensed and the non-condensed parts in vapor form and containing alltheir heat are conducted into a zone of the preliminary purifier, whichzone is free from any injurious counter-pressure and are subjected incirculation under automatic pressure regulation between these parts ofthe apparatus to a cooperative treatment, with the first part of thecrude vapors, and at the same time the steam-. inlet to any one-part ofthe apparatus being in circuit is regulated by a regulator, which islocated at a spot which is equally governed b pressure variation fromall of the parts 0 the apparatus being in circuit.

13. A process for the continuous distillation and rectification ofalcoholic liquids. wherein the crude alcohol vapors are divided into twoparts, one containing all fore-runnings, the other free fromforerunnings, the boiling hot phlegms of the first part purified fromthe fore-runnings are led in a fine spray or rain form and in onedirection into the second part of the crude vapors which is free fromfore-runnings, the vapors leaving the 'mixing compartment are r ectifiedand for the purpose of freeing the same of all odor and carried alongimpurities are at a possible highest temperature dephlegmated andcondensedand the'non-condensed parts in vapor form and containing alltheir heat are conducted into a zone of the preliminary purifier, whichzone is free from any injurious counter-pressure and are subjected incirculation under automatic pressure regulation between these parts ofthe apparatus to a cofiperative treatment with the first part of thecrude vapors, and at the same time the steam-inlet to any one-part ofthe apparatus being in circuit is regulated which is located at a spotwhich is equally governed by pressure variation from all of the parts ofthe apparatus being in circuit, and the proportion between the volume ofthe extracted fine-product and of the liquid respectively phlegms fiowininto the differ ent columns as well as o the flowing ofi' e I mew,

non-alcoholic liquid is regulated by e, &esigned my name this 14th dayof October, vice which governs the flow of the liquids 1908, in thepresence of two subscribing witaccording to the temperature whichpremesses.v veils in the zone subjected to the greatest VICTOR SLAVICEK.change of the temperature in the rectifying Witnesses: column. I ROBERTW. HEINGARTNER,

Intestimony whereof I have hereunto AUGUST FUGGER.

